Tag Archives: stability

Leaders in Cannabis Formulations: Part 4

By Aaron Green
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Natural cannabinoid distillates and isolates are hydrophobic oils and solids, meaning that they do not mix well with water and are poorly absorbed in the human body after consumption. Cannabinoid oils can be formulated into emulsions to form a fine suspension in water to improve bioavailability, stability and flavor. Vertosa is a cannabis infused ingredients company specializing in emulsion technologies. Their technology can be found in a range of CBD and THC containing beverages found on shelves today.

We spoke with Austin Stevenson, chief innovation officer at Vertosa, to learn more about emulsification technology and some of the challenges in testing cannabis infused beverages. Stevenson joined Vertosa in 2019 after spending time as a cannabis advisor at CanopyBoulder as an entrepreneur in residence. Prior to Vertosa, Stevenson ran the hemp and CBD analytical testing laboratory business unit for Eurofins.

Aaron Green: How did you get involved in the cannabis industry?

Austin Stevenson: I got involved in the cannabis industry nearly seven years ago, when I was an advisor to an accelerator in agriculture technology in Africa. I went to the MIT Innovation Laboratory, and I saw a whole bunch of farmers cultivating green leafy vegetables in the middle of the Kalahari Desert, which piqued my curiosity. I learned that it was all done via hydroponic indoor cultivation and freight containers. I got back to the US and put my detective hat on, and learned that it was really the cannabis industry that was driving innovation in terms of indoor and sustainable agriculture. At that point, I took it as an opportunity to dive in and started, again, as an advisor at an accelerator in Colorado. From there, I’ve been on the amazing cannabis journey.

Green: And how did you get involved with Vertosa?

Austin Stevenson, Chief Innovation Officer at Vertosa

Stevenson: I became an advisor at CanopyBoulder to a few software companies and got on the founding team there as well as at a few cultivation companies and other license types across the supply chain. Immediately before Vertosa, I ran the business unit for hemp and CBD testing at Eurofins, one of the world’s largest analytical chemistry laboratories, specializing in Ag Pharma. My clients were your traditional retailers: CVS, Kroger. Our team analyzed thousands, maybe hundreds of thousands of SKUs of infused products.

At one point I had to tell one of my clients at Eurofins, that all of their beverage SKUs were failing potency tests. Their supplements, OTC products, some of the confections, cosmetics, were all passing, but the beverages were failing potency testing. Cannabinoid ingredients were floating to the top, sinking to the bottom, even leaching into the can liners. It just wasn’t working, so we had to tell them that those beverages could not go to market. On this same day, I happened to run into my longtime friend and business partner in the industry (now Vertosa CEO) Ben Larson at a conference in Oakland, who was running the Gateway Incubator at the time, but had met our other partner and founder, Dr. Harold Han. Ben told me, “I have this PhD chemist, a surface chemist from BioRad. He’s been experimenting with techniques, taking cannabis oils and turning them into fast acting emulsions for beverages. I’d like for you to check it out because I’m considering building a business around this.” I said, “Alright, show me the technology. Let me take it back to the lab, analyze it, verify it, and then try it. See if it works.” Lo and behold, it did. I fell in love with the product. I saw the problem firsthand at my lab and now I saw a solution, so I knew that the next part of my cannabis journey would be to join Ben and Harold in building a business together focused on being the number one technology solving the problem of stability and potency for the infused beverage market.

Green: What is the core technology of Vertosa?

Stevenson: Our focus at Vertosa is being the best delivery mechanism for cannabinoids. That means that we have a portfolio of different technologies that we’re using to take cannabis oils and turn them into fast-acting liquid emulsions, as well as powder-based APIs. When we began, we were using nano-emulsification. We are using nanotechnology in the food space, with a few different methods for creating those nano-emulsions, to infuse a diverse range of different products – everything from seltzer waters to dealcoholized wines and teas.

Green: So, it’s a portfolio of products with the basic idea of encapsulating the oil into smaller components. Can you highlight some of the challenges when you were first developing the product with testing? My assumption is that it was relatively new for testing labs. How did you support method development with them so that you are accurately reporting cannabinoid content?

Stevenson: The biggest problem that we faced at Vertosa is that there’s no one size that fits all. The chemistry of an infused seltzer water is different than the chemistry of a dealcoholized wine. The reason is because, quite literally, the ingredients are different. They’re different products. When we’re making the emulsions for these beverages, all the ingredients have to be compatible – the ingredients in the emulsion as well as the ingredients in the beverage. We’ve had to design a portfolio of different emulsions for different beverage types to ensure compatibility in any scenario, otherwise there could be instability, causing separation between the emulsion and the ingredients.

Additionally, we’ve seen challenges in the packaging type as well as the manufacturing techniques, specifically sterilization, thermal processing, chemical treatment, or the lack thereof. These three core variables (ingredients, packaging, and manufacturing technique) are where all the challenges in potency testing arise. For example, you have an infused beverage that is going to be packaged in an aluminum can. There is a polarity between cannabinoids and the can aligners that ultimately could create leaching, or an absorption type of effect.

At Eurofins, we would see beverages that were supposed to contain CBD in the can but were testing at 0 milligrams, despite manufacturers confirming that they had added the CBD. All the CBD had been absorbed into the can liner. Our teams of method development chemists and management had learned to acid rinse the can liner so that we would be able to capture the cannabinoids and identify them. That was a step that we had to learn through trial and error, and we were able to bring this over and build upon this at Vertosa.

Here at Vertosa, the biggest challenge in the lab currently is that there aren’t consistent methods for analyzing beverages. Every lab has different standards, and the instrumentation hasn’t always been calibrated. To ensure that these low dose beverages are measured properly, you have an accurate LOQ to identify the cannabinoid content. Part of the challenge is that the analytical chemistry community has only started to collaborate here recently, literally in the last few months as the AOAC made a call to action for methods for beverage.

At Vertosa, we’ve had to work together with the labs and ask if they have a method for developing beverages. It’s a three-step approach: we send a lab the oil, the emulsion, and the finished product, and ensure that the accurate cannabinoid profile is being diluted across the entire chain to make sure that each step the instrumentation has been calibrated the correct way. We want to make sure that they calibrate it into the HPLC and that the correct cannabinoid profile is always consistent in the finished product. It’s a lot of intimate hand-holding with the labs.

Green: So, you took it upon yourself to go out and get the methods validated, anticipating the need for finished goods testing with your customers and partners?

Stevenson: That’s right. From the beginning, we understood that the problems we are setting out to solve are consistent potency testing and accurate dosing. We wanted to be able to say confidently that when you work with us, you’re going to pass potency tests every time. And if you don’t, we’re going to uncover the reasons why.

For us, we have been able to provide that consistent and reliable ingredient. And yes, there’s been stumbles along the way, but those stumbles are the learnings that make us better. In the beginning, we had just one formula but the chemistries of different beverages vary too much for that to work. We also know that packaging type and manufacturing processes play a role. So, we now have a portfolio of different emulsions, such as conventional, natural, and organic, that can work with any given varibale and that have verifiable potency.

We anchor ourselves to the promise that our clients will pass potency, because that’s the biggest problem most brands have.We know the ingredients inside and out – knowing how heat plays a role, how polyphenols play a role, how oxygen plays a role, and helping the labs and our brand partners succeed while minimizing all the risk and pain that they go through with failed potency. You’d be surprised how many people are using the wrong product in formulation. A new client will come to us frustrated after adding CBD isolate powder to their beverage and seeing it fail potency tests. That’s where we’re able to come in and correct the course.

Green: Someone comes in with a magic wand. What do they solve for you?

“Efficacy research is the most interesting aspect of industry research to me.”Stevenson: If I had a magic wand, I would use it to accelerate efficacy research to validate and verify specific cannabinoids/terpene formulas for targeted effects. In other words, I’d love to have a peer-reviewed, scientifically validated cannabis formula for any desired effect, like anxiety or pain relief, aid in sleep, or increased energy, for example. At Vertosa, we’re currently investing in third party academic research to empower our clients with validated information; however, it takes a lot of time, money, and effort conducting research and clinical trials. It’s a long but essential and beneficial process!

Green: What trends are you following in the industry?

Stevenson: In the world of edibles and ingestibles, I’m extremely interested in exploring onset times and bioavailability technologies, as well as trends in ingredients. More of our clients are interested in rapid onset times so that consumers feel the effects within minutes of consumption, removing some of the stereotypical hesitation around edibles and wondering when “it’ll hit.” It’s also fascinating to explore and integrate minor cannabinoids as well as active and functional ingredients and how they interact together in an ingestible.

I’m also extremely interested in keeping up with changing regulatory policy around consumption lounges and access in recently recreational states. Open consumption lounges are a fantastic solution to further normalizing cannabis usage and decentralizing alcohol in our culture, as consumer behavior is increasingly reflecting a move away from alcohol towards more health-conscious choices.

Green: What are you most interested in learning about?

Stevenson: Efficacy research is the most interesting aspect of industry research to me. Most of us cannabis professionals are passionate about the plant, and anecdotally know how cannabis can be used to improve quality of life. However, the scientific and academic community needs to see hard evidence. As we build the industry in a post-prohibition era, there is more access to research grants to evaluate the efficacy and safety of cannabis. The National Institute of Health (NIH) has identified four (4) key areas of cannabis research eligible for grant funding: (1) cannabinoid research (2) cannabidiol research (3) endocannabinoid system, ECS research, and (4) therapeutic effects of cannabinoids. It’s the latter two, ECS and therapeutic effects, that really spark my curiosity. At VERTOSA, we’re spending a lot of time and resources with our Scientific Advisory board to help accelerate this research, and I’m personally excited about the forthcoming discoveries we make, which will help our entire industry grow and thrive!

Bio-Rad Aspergillus PCR Test Gets AOAC Approval

By Cannabis Industry Journal Staff
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According to a press release published earlier this month, the Bio-Rad iQ-Check Aspergilllus Real-Time PCR Detection Kit has received AOAC International approval. The test covers detection for four different Aspergillus species: A. flavus, A. fumigatus, A. niger, and A. terreus.

The detection kit covers those Aspergillus species for testing in cannabis flower and cannabis concentrates, produced with our without solvents. The PCR detection kit was validated through the AOAC Research Institute’s Performance Tested Method Program. They conducted a study that resulted in “no significant difference” between the PCR detection kit and the reference method.

The iQ-Check Aspergillus Real-Time PCR Kit detects Aspergillus flavus, fumigatus, niger, and terreus in cannabis flower and cannabis concentrates.

The kit was evaluated on “robustness, product consistency, stability, inclusivity and exclusivity, and matrix studies,” the press release says. Bio-Rad also received approval and validation on the iQ-Check Free DNA Removal Solution, part of the workflow for testing cannabis flower.

The test kit uses gene amplification and real-time PCR detection. Following enrichment and DNA extraction, the test runs their PCR technology, then runs the CFX Manager IDE software to automatically generate and analyze results.

Bio’Rad has also recently received AOAC approval for other microbial testing methods in cannabis, including their iQ-Check Salmonella II, iQ-Check STEC VirX, and iQ-Check STEC SerO II PCR Detection Kits.

Leaders in Infused Products Manufacturing: Part 4

By Aaron Green
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Cannabis infused products manufacturing is quickly becoming a massive new market. With companies producing everything from gummies to lotions, there is a lot of room for growth as consumer data is showing a larger shift away from smokable products to ingestible or infused products.

This is the fourth article in a series where we interview leaders in the national infused products market. In this third piece, we talk with Stephanie Gorecki, vice president of product development at Cresco Labs. Stephanie started with Cresco in 2019 after transitioning from an award-winning career in traditional foods CPG. She now heads up product development where she manages R&D for Cresco, a multi-state operation with tremendous SKU variety.

Next week, we’ll sit down with Lisa McClung and Glenn Armstrong from Coda Signature. Stay tuned for more!

Aaron Green: Stephanie, how did you get involved at Cresco Labs?

Stephanie Gorecki: A few years ago, CBD became the most talked about ingredient in the food industry. CBD-infused food headlines appeared in most of the trade magazines. I have always been curious about working in the cannabis space, and not just with CBD, but THC and other cannabinoids. I researched technical seminars and came across the cannabis infused edibles short course put on by the Institute of Food Technologists.

Stephanie Gorecki, Vice President of Product Development at Cresco Labs

I attended the short course in April of 2019. I realized that to be hands-on with cannabis in the near future, I would need to join an organization that was already in the space. The space was highly regulated which meant that research in the mainstream food and beverage space was limited.

Immediately following that seminar, I began to look for opportunities near where I lived. That’s when I came across the Cresco Labs career opportunity. The Director of Food Science position appeared to be a good match. I applied for the position and went through the interview process. Approximately two months after attending that seminar, I joined Cresco Labs.

Aaron: Awesome! It’s a cool story. In your role, how do you think about developing products that differentiate in the market?

Stephanie: There are many opportunities for brand differentiation in cannabis right now. There is a focus on high bioavailability and water solubility and how that translates to onset times once consumed. Many of these technologies utilize ingredient technologies and systems that I have experience with from my past work in the flavor industry.

Gummies and jellies are a great infusion matrix to start with because of their shelf-life stability. There are a variety of formulation techniques that can be used to deliver on product differentiations. There is an abundance of flavor varieties, colors, processing steps and cannabinoid ratios that can be baked into a formula to make that product line unique.

Here in the cannabis space, SKU variety is essential. It’s exciting to be a part of a company where we develop products that appeal to a variety of customer wants and needs.

Aaron: In that vein, what’s your process then for creating a new product?

Stephanie: I’ll start with how we develop an edible. Most of my background is in this type of product development, but the same process is applied to how we develop and extract vape, topical, flower SKU, or ready-to-smoke type products. We follow a similar stage/gate process utilized by most CPG companies.

Marketing typically presents our product development team with a brief on a new concept based on how they’ve read the needs of the market. There are opportunities for us to come to marketing with ideas for innovation, too. The product development team regularly works in our processing facility, so we as a team are aware of the different capabilities of each state and production line. During the briefing phase, we determine what is needed to be achieved and the parameters that the team would like the new product to deliver on.

For edibles, we begin our development work at The Hatchery. The Hatchery is our non-infused product development space that we utilize outside of our processing facility. In this space, we have several pieces of pilot equipment that allow us to scale and create prototypes that are highly representative of what our finished product will look like. For vapes, flower SKUs and RTS (ready-to-smoke) products, development and processing trials happen within our cultivation center.

All infusions are conducted in our licensed processing center. We also conduct stability testing and analytical testing in-house on our products. Our analytical lab is amazing – we have talented chemists and the ability to run GCMS, HPLC, microbiological testing, and many other analytical tests that are important for ensuring consistency and product uniformity.

Aaron: Can you expand on a point about testing? How do you think about testing at the different points in your manufacturing or production process?

Stephanie: Testing comes in several forms. We focus heavily on analytical testing since that does not involve product consumption. Potency uniformity and consistency is critical for edibles. For infused products, we have one shot at hitting our potency – infusion science is extremely important for us. Our gummies and chocolates cannot be re-worked, so hitting our potency range on the first attempt is important. If we miss the target, the product has to be destroyed.

We have methods developed to conduct in-process potency testing where we can. With the processes and infusion methods that we have implemented, we are rarely outside of our targeted potency ranges.

Aaron: Okay, awesome, then, can you walk me through your experience with one of your most recent product launches?

Stephanie: We recently launched Mindy’s Dark Chocolate Peppermint Bark, a limited time offering for our Mindy’s chocolate line. There’s a series of commercialization trials that we will conduct prior to launch. We use these trials as an opportunity to train our production teams on the new manufacturing instructions and processes.

When it comes to launching products, our technical teams are very hands on with new product introductions. Since we cannot manufacture product in one state and ship it to another state, we have to build processing centers and secure the proper licenses in every state that we’d like to operate in. When we have a new product ready to launch in a new state, our team works with Operations on the tech transfer piece. We’re there on-site during launches to oversee and train on the entire process until our teams are comfortable with manufacturing and packaging the new SKUs.

We monitor launches carefully to ensure product looks as it should before and after leaving our facility for sale in licensed dispensaries across the state. When there are opportunities to optimize a process post-launch, we will do what we can to make the process work as well as possible for the teams producing our products.

Aaron: Okay, so next question is, how do you go about sourcing ingredients for your infused products?

Stephanie: We manufacture our oils and extracts in house, and then source other ingredients externally. We have a supplier quality assurance process for new supplier approval, and we have documentation needs that we need each supplier to be able to deliver on.

Several of our suppliers have invested in research and development of products that will help us to meet our deliverables in the cannabis industry. Our suppliers, at times, have provided applications support in order to help with our speed to market and early phase prototyping. These types of partnerships are essential to us being able to make quick modifications and decisions on ingredients such as flavors and colors.

Aaron: Can you give me an example of a challenge that you run into frequently? This could be a business challenge or a cannabis-related challenge.

 “I’m a scientist at heart. I look forward to more spending on cannabis research to show how THC and other cannabinoids can be used to treat a variety of conditions.”Stephanie: A big challenge for us and other multi-state cannabis operators are the variations in compliance regulations state-to-state. We have compliance managers in every state who work to ensure we are meeting all of the state regulations. Our packaging reviews are in-depth because of all the language that needs to be included on our packaging.

Each state needs its own packaging with proper compliance labeling. Some states require a cannabis warning symbol of a certain type. If we sell Mindy’s Gummies in 8 flavors and THC mg SKUs in four states, that is 32 different pieces of artwork that need to be managed and cross-checked for accuracy. We have 32 separate pieces of packaging for this one line of products. We have many lines of products with multiples strains (flower and vapes) and flavors (edibles).

Aaron: You mentioned packaging, do you do all of your packaging in house?

Stephanie: We design our packaging artwork in-house. We have a creative team who works on our product artwork, and then a team of cross-functional members tasked with packaging editing and review. Packaging reviews go through multiple rounds before being released for printing. We source a variety of packaging depending on the needs of the product going into the packaging. For edibles, our packaging has to be opaque. Product cannot be seen through the packaging in most states. This is great for our products that are made with natural colors that may be light sensitive.

All of our packaging needs to be child resistant. This limits the amount of packaging variety that we have, but this is a big opportunity for packaging developers. We want and need more sustainable forms of packaging that are differentiated from other packaging forms currently on the market.

Aaron: What trends are you following in the industry personally?

Stephanie: Cannabis trends that are of interest to me personally are fast-onset and water solubility technology. There have also been many discussions surrounding minor cannabinoids and how those can be blended together to drive customer experience.

There are traditional food trends that also impact how we formulate. Our Mindy’s Edibles line is flavor forward. The flavors are sophisticated. In the Mindy’s line, you won’t find a generic orange or grape flavor. Instead, you’ll find a Lush Black Cherry or Cool Key Lime Kiwi Flavor. This flavor development work starts with Mindy Segal, who is the face and talented James Beard award-winning chef behind our Mindy’s Edibles line of products.

Aaron: Okay, so the last question I have for you is, what are you interested in learning more about?

Stephanie: I’m a scientist at heart. I look forward to more spending on cannabis research to show how THC and other cannabinoids can be used to treat a variety of conditions. People use cannabis for many reasons: to relax, to ease aches or pains, etc. It’s exciting to lead part of our technical team during a period of time where cannabis is rapidly growing and is of great interest and increasing acceptance across our country and in the world.

Aaron: Okay. So that’s it. That’s the end of the interview!

Leaders in Extraction & Manufacturing: Part 2

By Aaron Green
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Cannabis extraction and manufacturing is big business in California with companies expanding brands into additional states as they grow. This is the second article in a series where we interview leaders in the California extraction and manufacturing industry from some of the biggest and most well-known brands. Click here to see Part 1.

In this week’s article we talk with Matthew Elmes, director of product development at Cannacraft. After cutting his teeth in academic and industry research, Matthew was approached by Cannacraft leadership to bring a new perspective to their product development efforts. The interview with Matthew was conducted on July 22, 2020.

Next week, we’ll interview Joaquin Rodriguez, chief operating officer at GenX BioTech. Stay tuned for more!

Aaron Green: Hi Matthew, and thank you for taking the time to chat today, I understand you have a busy schedule!

Matthew Elmes: Thanks – yeah, last week was pretty insane!

Aaron: Well, I’m happy we found a chance to put this together. Let’s start from the beginning. How did you get involved at Cannacraft?

Matthew Elmes, director of product development at Cannacraft

Matthew: I did my Ph.D in biochemistry at Stony Brook University on cannabinoid intracellular transport and metabolism. I then did a post-doc with Artelo Biosciences in endocannabinoid system modulation. While I was doing my post-doctoral research, Dennis Hunter, co-founder of Cannacraft, had learned about my work and reached out to offer me a position.

Aaron: Awesome, that’s a great feeling when people are reaching out to you! The next questions here will be focused on product development and manufacturing. What is your decision process for launching a new product?

Matthew: We do our best to anticipate what the market will want. A lot of our new product development comes from improving our current products. Things like improving stability, shelf-life and reducing bitterness. For brand-new products and technologies, we first get a lot of feedback from the marketing and sales teams and will then go into a planning session to decide what is feasible and what is not prior to moving forward.

Aaron: Do you personally get involved in manufacturing? Tell me about your process there.

Matthew: I do get involved in manufacturing. My main inputs are figuring out how much cannabis oil to use to hit a target potency around the size of a batch. This is the type of thing I do for all our beverage products like HiFi Hops, our Satori line of infused edibles, and the various gummy products sold under our brands Absolute Xtracts and Care By Design.

Aaron: Are you developing new products internally?

Matthew: For the most part we develop everything internally. We are very vertically integrated here at Cannacraft and we extract all of our oil in house. I don’t do the oil extractions myself. Most of our stuff is supercritical carbon dioxide extraction, but we have hydrocarbon and cryoethanol extraction facilities opening soon. For our gummies, we use distillate oils for the best flavor and for our droppers/vapes we use full-spectrum oils for a more sophisticated array of effects.

Aaron: In product development, what does getting stuck look like for you?

Matthew: Getting stuck happens a lot! You know, strict regulations make it challenging to source ingredients. Foods we’d like to source for a product are often too high in pesticides or heavy metals for the cannabis regulations. What’s good enough for the grocery store is very often not good enough to be compliant in the California cannabis industry. Fruits that are totally free from pesticides are hard to find. Our edibles brand Satori Chocolates actually might be the only player in the entire California cannabis industry that uses real whole fruit in our products rather than something artificial or a processed fruit paste. We actually had to source our strawberries from Italy to find ones that were both compliant in metals/pesticides and tasted good enough to meet our high standards! The same sort of challenges apply to sourcing biomass for oils.

Aaron: If you get stuck is it usually the same place? Or is it different each time?

Matthew: We’re so diversified. We have lots of different products. The process for each one can have its own issues. The problems you encounter with cannabis beverages are not the same ones that you’ll encounter with vapes, edibles, topicals or sublinguals, etc. We are one of the oldest players in the California cannabis industry (CannaCraft was founded in 2014, well before regulated recreational cannabis was a thing) so we have the advantage of working on all these issues for years longer than most of our competitors and we have largely figured out all the major ‘kinks’ already. A big part of it is also that we have assembled a great team of food scientists, chemical engineers, chemists, legal and regulatory experts, all with diverse specialties that allows us to quickly address any new ‘stucks’ and be fully confident in all of our products.

Aaron: Feel free to answer the next question however you like. What does your magic helper look like?

Matthew: I would love a magic helper! What would a magic helper look like to me? I think my magic helper is a recent undergrad with lab experience. I would have them take care of a lot of the quality and lab day to day activities. My responsibilities often make me too stuck to the computer screen where I don’t have time to get to all the experiments that I’d like to do…a trained magic helper could physically perform those experiments for me!

Aaron: OK, and now for our final question! What are you following in the market and what do you want to learn about?

Matthew: I am personally really interested in yeast grows and cannabinoid synthesis from biological organisms. We stick to only natural plant-derived cannabinoids for all our products, but it’s a new field that’s just fascinating to me. I also think that minor cannabinoids will have a bigger place in coming years. In particular I have my eye on THCV, ∆8-THC, CBG and THCP. THCP is a phytocannabinoid that was just discovered a year ago and exhibited very potent effects in preclinical models, but no one has been able to produce and purify it in appreciable amounts yet. We already manufacture and sell a ∆8-THC vape cart under our ABX brand, but for the others keep an eye out for new product announcements from us that are on the horizon.

Aaron: Well, that brings us to the end of the interview Matthew, this is all awesome feedback for the industry. Thanks so much for your time and insights into product development in the cannabis industry.

Matthew: Thanks, take care!

Multi-Element Analysis Using ICP-MS: A Look at Heavy Metals Testing

By Cannabis Industry Journal Staff
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Across the country and across the world, governments that legalize cannabis implement increasingly rigorous requirements for laboratory testing. Helping to protect patients and consumers from contaminants, these requirements involve a slew of lab tests, including quantifying the levels of microbial contaminants, pathogens, mold and heavy metals.

Cannabis and hemp have a unique ability to accumulate elements found in soil, which is why these plants can be used as effective tools for bioremediation. Because cannabis plants have the ability to absorb potentially toxic and dangerous elements found in the soil they grow in, lab testing regulations often include the requirement for heavy metals testing, such as Cadmium, Lead, Mercury, Arsenic and others.

In addition to legal cannabis markets across the country, the USDA announced the establishment of the U.S. Domestic Hemp Production Program, following the enactment of the 2018 Farm Bill, essentially legalizing hemp. This announcement comes with information for hemp testing labs, including testing and sampling guidelines. While the information available on the USDA’s website only touches on testing for THC, required to be no greater than 0.3% dry weight concentration, more testing guidelines in the future are sure to include a discussion of heavy metals testing.

Table 1. ICP-MS operating conditions (shaded parameters were automatically optimized during start up for the HMI conditions).

In an application note produced by Agilent Technologies, Inc., the Agilent 7800 ICP-MS was used to analyze 25 elements in a variety of cannabis and hemp-derived products. The study was conducted using that Agilent 7800 ICP-MS, which includes Agilent’s proprietary High Matrix Introduction (HMI) system. The analysis was automated  by using the Agilent SPS 4 autosampler.

Instrumentation

The instrument operating conditions can be found in Table 1. In this study, the HMI dilution factor was 4x and the analytes were all acquired in the Helium collision mode. Using this methodology, the Helium collision mode consistently reduces or completely eliminates all common polyatomic interferences using kinetic energy discrimination (KED).

Table 2. Parameters for microwave digestion.

As a comparison, Arsenic and Selenium were also acquired via the MassHunter Software using half-mass correction, which corrects for overlaps due to doubly charged rare earth elements. This software also collects semiquantitative or screening data across the entire mass region, called Quick Scan, showing data for elements that may not be present in the original calibration standards.

SRMs and Samples

Standard reference materials (SRMs) analyzed from the National Institute of Standards and Technology (NIST) were used to verify the sample prep digestion process. Those included NIST 1547 Peach Leaves, NIST 1573a Tomato Leaves and NIST 1575 Pine Needles. NIST 1640a Natural Water was also used to verify the calibration.

Figure 1. Calibration curves for As, Cd, Pb, and Hg.

Samples used in the study include cannabis flower, cannabis tablets, a cannabidiol (CBD) tincture, chewable candies and hemp-derived cream.

Sample Preparation

Calibration standards were prepared using a mix of 1% HNO3 and 0.5% HCl. Sodium, Magnesium, Potassium, Calcium and Iron were calibrated from 0.5 to 10 ppm. Mercury was calibrated from 0.05 to 2 ppb. All the other elements were calibrated from 0.5 to 100 ppb.

Table 3. Calibration summary data acquired in He mode. Data for As and Se in shaded cells was obtained using half mass correction tuning.

After weighing the samples (roughly 0.15 g of cannabis plant and between 0.3 to 0.5 g of cannabis product) into quartz vessels, 4 mL HNO3 and 1 mL HCl were added and the samples were microwave digested using the program found in Table 2.

HCI was included to ensure the stability of Mercury and Silver in solution. They diluted the digested samples in the same acid mix as the standards. SRMs were prepared using the same method to verify sample digestion and to confirm the recovery of analytes.

Four samples were prepared in triplicate and fortified with the Agilent Environmental Mix Spike solution prior to the analysis. All samples, spikes and SRMs were diluted 5x before testing to reduce the acid concentration.

Calibration

Table 4. ICV and CCV recovery tests. Data for As and Se in shaded cells was obtained using half mass correction tuning.

The calibration curves for Arsenic, Cadmium, Lead and Mercury can be found in Figure 1 and a summary of the calibration data is in Table 3. For quality control, the SRM NIST 1645a Natural Water was used for the initial calibration verification standard.  Recoveries found in Table 4 are for all the certified elements present in SRM NIST 1640a. The mean recoveries and concentration range can also be found in Table 4. All the continuing calibration solution recoveries were within 10% of the expected value.

Internal Standard Stability

Figure 2 highlights the ISTD signal stability for the sequence of 58 samples analyzed over roughly four hours. The recoveries for all samples were well within 20 % of the value in the initial calibration standard.

Figure 2. Internal standard signal stability for the sequence of 58 samples analyzed over ~four hours.

Results

In Table 5, you’ll find that three SRMs were tested to verify the digestion process. The mean results for most elements agreed with the certified concentrations, however the results for Arsenic in NIST 1547 and Selenium in both NIST 1547 and 1573a did not show good agreement due to interreferences formed from the presence of doubly-charged ions

Table 5. Mean concentrations (ppm) of three repeat measurements of three SRMs, including certified element concentrations, where appropriate, and % recovery.

Some plant materials can contain high levels of rare earth elements, which have low second ionization potentials, so they tend to form doubly-charged ions. As the quadrupole Mass Spec separates ions based on their mass-to-charge ratio, the doubly-charged ions appear at half of their true mass. Because of that, a handful of those doubly-charged ions caused overlaps leading to bias in the results for Arsenic and Selenium in samples that have high levels of rare earth elements. Using half mass correction, the ICP-MS corrects for these interferences, which can be automatically set up in the MassHunter software. The shaded cells in Table 5 highlight the half mass corrected results for Arsenic and Selenium, demonstrating recoveries in agreement with the certified concentrations.

In Table 6, you’ll find the quantitative results for cannabis tablets and the CBD tincture. Although the concentrations of Arsenic, Cadmium, Lead and Cobalt are well below current regulations’ maximum levels, they do show up relatively high in the cannabis tablets sample. Both Lead and Cadmium also had notably higher levels in the CBD tincture as well.

Table 6. Quantitative data for two cannabis-related products and two cannabis samples plus mean spike recovery results. All units ppb apart from major elements, which are reported as ppm.

A spike recovery test was utilized to check the accuracy of the method for sample analysis. The spike results are in Table 6.

Using the 7800 ICP-MS instrument and the High Matrix Introduction system, labs can routinely analyze samples that contain high and very variable matrix levels. Using the automated HMI system, labs can reduce the need to manually handle samples, which can reduce the potential for contamination during sample prep. The MassHunter Quick Scan function shows a complete analysis of the heavy metals in the sample, including data reported for elements not included in the calibration standards.

The half mass correction for Arsenic and Selenium allows a lab to accurately determine the correct concentrations. The study showed the validity of the microwave sample prep method with good recovery results for the SRMs. Using the Agilent 7800 ICP-MS in a cannabis or hemp testing lab can be an effective and efficient way to test cannabis products for heavy metals. This test can be used in various stages of the supply chain as a tool for quality controls in the cannabis and hemp markets.


Disclaimer: Agilent products and solutions are intended to be used for cannabis quality control and safety testing in laboratories where such use is permitted under state/country law.

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EVIO Labs Florida Achieves ISO17025:2017 Accreditation

By Aaron G. Biros
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EVIO Labs Florida received their ISO 17025:2005 accreditation in February of 2018. Last week, EVIO Labs Florida announced via a press release that they completed their ISO 17025:2017 accreditation and received a certification from AOAC International. The accreditation helped them to further expand their testing scope to shelf life and stability testing, the ability to detect harmful bacteria and calculate degradation in samples.

The certification that they received from AOAC helps verify their ability to conduct accurate and fair 3rd party testing, meeting Florida’s requirements for the market. Back when the laboratory first started in 2017, there were no requirements for lab testing cannabis products under Florida’s regulations.

Chris Martinez
Chris Martinez, co-founder and president of EVIO Labs Florida

Upon expanding to their Gainesville location in November last year and getting accredited to ISO 17025:2017 last week, EVIO Labs Florida expects the new location to be compliant and operational by April 2019, in preparation for the state’s new regulations. “Our team has worked diligently to maintain our stance as the Gold Standard in Cannabis Testing,” says Chris Martinez, co-founder and president of EVIO Lab Florida. “The ability to obtain the recent ISO 17025:2017 and AOAC certification is a testament to our dedication in maintaining public safety and product integrity in an ever-growing industry.”

Martinez is also presenting during the 2ndAnnual Cannabis Labs Virtual Conference on April 2, where he will discuss how EVIO Labs Florida began as a laboratory and how they were able to expand to a second location and grow their market presence in Florida. Click here to register for his talk.